Acetic Acid → HCID 2775935、化合物

HRID 635801ノート

反応式

HRID 635801 の反応式
[S:1]=[C:2]1[CH:7]=[N:6][NH:5][C:4](=[O:8])[NH:3]1.CI.[OH-].[Na+].[C:13](O)(=O)C>O>[CH3:13][S:1][C:2]1[CH:7]=[N:6][NH:5][C:4](=[O:8])[N:3]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 14162865-Thioxo-4,5-dihydro-1,2,4-triazin-3(2H)-one

生成物 1

HCID 2775935HCID 2775935、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The compound 9a (30 g, 232 mmol) and CH3I (15.9 ml, 255 mmol) are placed in 300 ml of water. 18.6 g of NaOH (465 mmol) are added and the mixture is stirred for 1 h at room temperature. The reaction mixture, cooled on a bed of ice, is neutralized using 27 ml of acetic acid and then extracted with dichloromethane. The organic phases are dried (MgSO4) and then concentrated to dryness. After recrystallizing from ether, 29.9 g of compound 9b are isolated.

後処理

  1. temperatureThe reaction mixture, cooled on a bed of ice
  2. extractionextracted with dichloromethane
  3. dry with materialThe organic phases are dried (MgSO4)
  4. concentrationconcentrated to dryness
  5. customAfter recrystallizing from ether, 29.9 g of compound 9b
  6. customare isolated

出典と根拠

ORDレコード
ord-727fbd0710e5469f87d70ea172070feb
出典データセット
uspto-grants-2001_02
特許番号
US06191130B1

反応ノート

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